CA2748760A1 - Method for producing an anti-infective coating on implants - Google Patents

Method for producing an anti-infective coating on implants Download PDF

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Publication number
CA2748760A1
CA2748760A1 CA2748760A CA2748760A CA2748760A1 CA 2748760 A1 CA2748760 A1 CA 2748760A1 CA 2748760 A CA2748760 A CA 2748760A CA 2748760 A CA2748760 A CA 2748760A CA 2748760 A1 CA2748760 A1 CA 2748760A1
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CA
Canada
Prior art keywords
oxide layer
implants
metal
titanium
infective
Prior art date
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Granted
Application number
CA2748760A
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French (fr)
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CA2748760C (en
Inventor
Hans-Georg Neumann
Cornelia Prinz
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DOT GmbH
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DOT GmbH
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Publication of CA2748760C publication Critical patent/CA2748760C/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/306Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104Silver, e.g. silver sulfadiazine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Veterinary Medicine (AREA)
  • Dermatology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Public Health (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Materials For Medical Uses (AREA)
  • Prostheses (AREA)

Abstract

The invention relates to a method for producing an anti-infective coating on implants that contain titanium or are composed of titanium. The aim of the invention is to provide a coating method with which it is possible, for implants made of titanium or that contain titanium, to combine the optimization of the mechanical properties achieved with the anodic oxidation type II
with the optimization of the anti-infective properties. According to the invention, the implants are anodically oxidized in an alkali-ne solution, then metal having anti-infective properties is electrodeposited on said surface, and afterwards the oxide layer containing metal is solidified.

Description

Method for producing an anti-infective coating on implants Description [0001] The invention relates to a method for producing an anti-infective coating on implants, that contain titanium or are composed of titanium.

State of the art [0002] From DE 10243132 B4 is known to provide implants made of titanium or titanium alloys with a titanium oxide coating, in which metal ions such as silver and copper are homogeneously distributed, by using a sol-gel method. For the mechanical stabilization and densification of said coating a heat treatment is applied after drying. By means of heating to about 500 C a ceramization of the coating takes place. For the implants the heat treatment has the disadvantage that it results in a loss of strength. Therefore, it is not suitable for implants which must have high fatigue strength.
[0003] It is known that an anodic oxidation type II of titanium results in a greater hardness and higher fatigue strength. In DE 20020649 U1 this coating is also described as an anti-infective coating because of its smooth surface, besides silver and copper. However, it is not possible to produce a sufficiently adherent coating of silver or copper on an anodic oxidation type II coating.

Disclosure of the invention [0004] The invention is based on the object to provide a coating method by means of which it is possible for implants made of titanium or which contain titanium to combine the optimization of the mechanical properties achieved by the anodic oxidation type II with the optimization of the anti-infective properties.
[0005] This object is solved in that the implants are oxidized anodically in an alkaline solution, then metal having anti-infective properties is electrodeposited on the surface, and afterwards the metal-containing oxide layer is solidified.
[0006] In the anodic oxidation a conversion layer containing oxygen and optionally other atoms, and a porous titanium oxide layer having a sufficient conductivity, which is electrically conductive in the pores, such that metal can be electrode posited in it, can be formed. By blasting, e.g. with glass beads, the metal-containing oxide layer is solidified, and more weakly bound oxide and metal particles are removed or more intensely connected with each other and with the surface of the implant.
[0007] There is provided a method for the combined modification of implants containing titanium or consisting of titanium, wherein in the first step a porous oxide layer is formed by anodic spark discharge in strongly alkaline electrolytes, in the second step the galvanic charge of metal into the porous layer takes place, and in a third step the metal-enriched oxide layer is solidified by blasting and can be more or less eliminated by removing more weakly bound oxide or metal particles or by connecting said particles more intensely with each other and the implant.
[0008] The elution of the metal starting under physiological conditions may be adjusted in regard to its concentration by variation of the mean metal coating of the implant surface, so that an antimicrobial or rather antibacterial action without any substantial damage to the cells of the surrounding body tissue is achieved. In particular copper, silver and zinc are suitable as metals. In the case of the metal copper there can be additionally expected an improved blood flow of the newly formed body tissue due to the catalytic effect on the angiogenesis. The thickness of the metal-containing layer is advantageously 8 -15 m, preferably 10 m.
[0009] Solidifying the metal-containing oxide layer is advantageously carried out by blasting with glass beads.

Brief Description of the Figures [0010] Figure 1 Partially copper-coated TiAIV-surface [0011] Figure 2 Development of cell number of staphylococcus aureus ATCC
25923 after culture on a partially copper-coated TiAIV-surface Carrying out the invention [0012] In the following the invention is explained in more detail by way of an example.
[0013] Example 1: Coating [0014] TiAI6V4-samples are coated with a porous oxide layer according to the principle of anodic spark discharge in a strongly alkaline electrolyte. For that, 50 g NaOH are dissolved in 500 ml of distilled water. In the solution heated to 40 C, the anodic spark oxidation of the titanium sample is conducted by slowly increasing the voltage to 40 volt. Then, copper from a saturated copper acetate solution is added into the porous oxide layer by means of cathode deposition. The resulting copper-enriched oxide layer is partially removed by glass bead blasting, and the copper contained in it is almost completely incorporated in an island-like manner into the sample surface (Figure 1).
[0015] Example 2: Description of the antibacterial mechanism [0016] For testing the antibacterial action investigations were performed on clinically relevant bacterial strain staphylococcus aureus ATCC25923. For that, TiAIV-cylinders with a diameter of 8 mm and a length of 20 mm were coated with copper according to Example 1, and outsourced at 37 C for various times in 6 ml of a PBS buffer solution which had been vaccinated with 150 l of bacterial suspension. Thereafter, the concentration of the living bacteria on the cylinders and in the solution was determined by plating on agar culture media and by outsourcing (48 h) at 30 C.
Even after only 4 hours no living bacteria were found on the cylinders and after 24 hours only very few living bacteria were found in the buffer solution (Figure 2).

Claims (6)

1. A method for producing an anti-infective coating on implants, which contain titanium or are composed of titanium, characterized by the following steps - formation of a porous oxide layer by anodic oxidation in an alkaline solution, such that the conductivity in the pores enables an electrodeposition, - electrodeposition of a metal with anti-infective properties, - solidification of said metal-containing oxide layer by blasting.
2. The method according to claim 1, characterized in that the electrolyte for said anodic oxidation contains sodium hydroxide solution.
3. Method according to claim 1 or 2, characterized in that said electrolyte contains soda water glass.
4. The method according to claim 1, characterized in that copper, silver and/or zinc are added into said porous oxide layer.
5. The method according to claim 1, characterized in that said metal-containing oxide layer is blasted with glass beads.
6. The method according to claim 1, characterized in that the thickness of said oxide layer is 8 - 15 µm.
CA2748760A 2009-01-05 2010-01-04 Method for producing an anti-infective coating on implants Expired - Fee Related CA2748760C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP09100006A EP2204199B1 (en) 2009-01-05 2009-01-05 Method for manufacturing an anti-infection coating on implants
EP09100006.7 2009-01-05
PCT/EP2010/050010 WO2010076338A1 (en) 2009-01-05 2010-01-04 Method for producing an anti-infective coating on implants

Publications (2)

Publication Number Publication Date
CA2748760A1 true CA2748760A1 (en) 2010-07-08
CA2748760C CA2748760C (en) 2015-07-21

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Family Applications (1)

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CA2748760A Expired - Fee Related CA2748760C (en) 2009-01-05 2010-01-04 Method for producing an anti-infective coating on implants

Country Status (9)

Country Link
US (1) US8828552B2 (en)
EP (1) EP2204199B1 (en)
JP (1) JP5647145B2 (en)
CN (1) CN102271721B (en)
AT (1) ATE530205T1 (en)
AU (1) AU2010203260B9 (en)
CA (1) CA2748760C (en)
ES (1) ES2376539T3 (en)
WO (1) WO2010076338A1 (en)

Cited By (1)

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EP2693978A2 (en) * 2011-04-01 2014-02-12 Washington State University Researchfoundation Materials with modified surfaces and methods of manufacturing

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TWI400100B (en) * 2010-09-29 2013-07-01 Metal Ind Res & Dev Ct Medical equipment and manufacturing methods thereof
KR101278740B1 (en) 2012-02-17 2013-06-25 영남대학교 산학협력단 Implants comprising water glass coating layer and preparation method thereof
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US10064273B2 (en) 2015-10-20 2018-08-28 MR Label Company Antimicrobial copper sheet overlays and related methods for making and using
AU2017211214A1 (en) 2016-01-25 2018-07-12 Smith & Nephew, Inc. Orthopaedic implant
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CN106420119B (en) * 2016-11-29 2017-10-31 淮阴工学院 A kind of manufacturing process of high antibiotic property titanium alloy artificial hip joint
WO2018187758A1 (en) * 2017-04-07 2018-10-11 The Board Of Trustees Of The University Of Illinois Directed plasma nanosynthesis (dpns) methods, uses and systems
CN107893252A (en) * 2017-11-22 2018-04-10 四川大学 Titanium base material surface has in-situ preparation method and its application of the bioactivity coatings of soft tissue seal
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2693978A2 (en) * 2011-04-01 2014-02-12 Washington State University Researchfoundation Materials with modified surfaces and methods of manufacturing
EP2693978A4 (en) * 2011-04-01 2014-11-05 Univ Washington State Res Fdn Materials with modified surfaces and methods of manufacturing
US9440002B2 (en) 2011-04-01 2016-09-13 Washington State University Materials with modified surfaces and methods of manufacturing

Also Published As

Publication number Publication date
ATE530205T1 (en) 2011-11-15
CA2748760C (en) 2015-07-21
WO2010076338A1 (en) 2010-07-08
EP2204199B1 (en) 2011-10-26
AU2010203260B2 (en) 2013-10-17
AU2010203260A1 (en) 2011-07-14
JP2012514483A (en) 2012-06-28
CN102271721A (en) 2011-12-07
JP5647145B2 (en) 2014-12-24
US8828552B2 (en) 2014-09-09
CN102271721B (en) 2014-12-10
EP2204199A1 (en) 2010-07-07
US20120024712A1 (en) 2012-02-02
ES2376539T3 (en) 2012-03-14
AU2010203260B9 (en) 2013-10-31

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